CN116457430A - 液体施加的隔音组合物 - Google Patents

液体施加的隔音组合物 Download PDF

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CN116457430A
CN116457430A CN202180075852.5A CN202180075852A CN116457430A CN 116457430 A CN116457430 A CN 116457430A CN 202180075852 A CN202180075852 A CN 202180075852A CN 116457430 A CN116457430 A CN 116457430A
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wax
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I·D·罗伯森
M·W·莱昂纳多
R·E·德鲁姆赖特
J·C·勃林
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Dow Global Technologies LLC
Rohm and Haas Co
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Abstract

本发明涉及一种组合物，该组合物包含以下物质的含水分散体：丙烯酸聚合物颗粒；石蜡；石墨颗粒；和增量剂颗粒。该组合物可用于制备用于液体施加的隔音应用的具有低水吸收的涂层。

Description

液体施加的隔音组合物
背景技术
本发明涉及适用于液体施加的隔音应用的组合物，更具体地，涉及形成具有优异抗水性的涂层的组合物。
阻尼材料用于刚性结构的减振以降低噪声。在机动车辆中，有以下两种主要的减震技术占主导地位：沥青垫和液体施加的来源于水性胶乳的隔音(LASD)涂层。沥青垫是20世纪中广泛使用的低成本替代品，表现出相对较差的阻尼性能，并且需要费力的手动应用。另一方面，LASD涂层已经获得了显著的市场份额，因为它们可以通过机械手喷雾技术快速施加。此外，LASD涂层表现出更好的阻尼特性、环境、健康和安全性(EH&S)曲线，以及较低的密度。一起，这些益处已导致机动车OEM越来越多地采用LASD用于噪声振动和危险(NVH)管理，超过现有的沥青垫。WO 2018/062546A1描述适于减振应用的聚合物颗粒的含水分散体。尽管报告了改善的起泡抑制，但未描述抗水性。本领域仍然需要开发具有与沥青垫相当的优异抗水性的LASD涂层。抗水LASD涂层可能有助于客户采用该技术。此外，改进的抗水性可以使LASD涂层用于新的应用领域，例如车辆的轮舱内。因此，开发一种聚合物颗粒的含水分散体将是本领域的一个进步，该含水分散体可以配制成抗水的，表现出优异外观并保持高减振性能的LASD涂层。
发明内容
本发明通过提供一种组合物解决了本领域中的需求，所述组合物包含以下物质的含水分散体：丙烯酸聚合物颗粒，所述丙烯酸聚合物颗粒具有50nm至500nm范围内的z平均粒度和-25℃至30℃范围内的计算Tg；石蜡；增量剂颗粒；和流变改性剂；其中所述组合物的颜料体积浓度在40至70的范围内；其中当不在剪切条件下时，所述组合物的布氏粘度在200,000cP至20,000,000cP的范围内。本发明的组合物可用于减少用于LASD应用的涂层中的水吸收。
具体实施方式
本发明是一种组合物，所述组合物包含以下物质的含水分散体：丙烯酸聚合物颗粒，所述丙烯酸聚合物颗粒具有50nm至500nm范围内的z平均粒度和-25℃至30℃范围内的计算Tg；石蜡；增量剂颗粒；和流变改性剂，其中所述组合物的颜料体积浓度在40至70的范围内；其中当不在剪切条件下时，所述组合物的布氏粘度在200,000cP至20,000,000cP的范围内。
如本文所用，术语丙烯酸聚合物颗粒(可替代地，丙烯酸胶乳颗粒)是指丙烯酸或苯乙烯-丙烯酸聚合物颗粒。聚合物颗粒优选地在环境温度下成膜；因此，聚合物颗粒的通过Fox公式计算的Tg优选地为不大于30℃、优选不大于20℃以及更优选不大于5℃；并且不低于-25℃，更优选不低于-10℃。优选地，聚合物颗粒包含甲基丙烯酸甲酯(MMA，Tg＝105℃)或苯乙烯(STY，Tg＝100℃)和选自以下的至少一种单体的结构单元：丙烯酸乙酯(EA，Tg＝-22℃)、丙烯酸丁酯(BA，Tg＝-54℃)、丙烯酸2-乙基己酯(2-EHA，Tg＝-70℃)和丙烯酸2-丙基庚酯(2-PHA，Tg＝-68℃)。
术语“结构单元”在本文中用于描述所述单体在聚合后的残余物。例如，MMA的结构单元如下说明：
其中虚线表示结构单元与聚合物主链的连接点。
聚合物颗粒优选地包含0.1重量％、更优选0.2重量％、以及最优选0.3重量％至6重量％、更优选至4重量％、以及最优选至3重量％的烯键式不饱和酸单体(诸如羧酸单体和磷酸单体)的结构单元。合适的羧酸单体的示例包括丙烯酸、甲基丙烯酸和衣康酸；合适的磷酸单体的示例包括醇的膦酸酯和磷酸二氢酯，其中醇含有可聚合的乙烯基或烯基或被可聚合的乙烯基或烯基取代。优选的磷酸二氢酯是丙烯酸羟烷基酯或甲基丙烯酸羟烷基酯的磷酸酯，包括甲基丙烯酸磷酸乙酯(PEM)和甲基丙烯酸磷酸丙酯。
基于组合物的重量，聚合物颗粒的浓度优选地在10重量％至25重量％的范围内。丙烯酸聚合物颗粒优选地具有通过动态光散射测量的在80nm至250nm范围内的z平均粒度。在一个方面，丙烯酸聚合物具有10,000g/mol至40,000g/mol范围内的数均分子量，如通过下文详述的凝胶渗透色谱法所测量。
石蜡是具有10个至40个乙烯重复单元的聚乙烯：
(CH2CH-2)n，
其中n为10至40。基于聚合物颗粒的重量，石蜡的浓度在优选1重量％、更优选2重量％以及最优选3重量％至优选15重量％、更优选至10重量％的范围内。合适的石蜡的商业示例包括Michem乳液47950、Michem lube 723和Aquacer乳液593，它们是用非离子表面活性剂稳定的石蜡水乳液。
该组合物还可以包含较高分子量(150个至1500个重复单元)的聚乙烯(PE)蜡或聚丙烯(PP)蜡。基于石蜡和较高分子量聚乙烯蜡或聚丙烯蜡的重量，较高分子量PE或PP(如果使用的话)的浓度优选地在5重量％至35重量％的范围内。石蜡/PE共混物乳液的商业示例包括Michem 62330和Michem 66035石蜡/PE蜡共混物乳液。
该组合物还包含增量剂颗粒，其通常具有1μm至50μm范围内的中值直径平均(D50)粒度。合适的增量剂(在本领域中也称为填料)的示例包括碳酸钙；二氧化硅；氧化铝；高岭土；粘土；滑石；石墨；云母；硅藻土；玻璃粉末、纤维或微球；氢氧化铝；珍珠岩；硫酸钡；碳酸镁；钙二水合物；岩棉；硅灰石；沸石；陶瓷和热塑性微球；聚合物纤维和交联橡胶颗粒。该组合物的颜料体积浓度(PVC)在40(优选50)至70(优选至65)的范围内。使用下式计算PVC：
其中颜料是指遮光颜料，诸如二氧化钛、氧化锌和氧化锆；并且粘合剂固体是指聚合物的来自将遮光颜料和增量剂颗粒粘合在一起的聚合物颗粒的含水分散体的贡献。该组合物优选地包含小于5PVC，更优选0PVC的遮光颜料。该组合物有利地包含其他添加剂，诸如流变改性剂、消泡剂、表面活性剂和马铃薯淀粉。
如以下实施例所证明，由本发明的组合物产生的涂层显示出水敏感性的显著降低，这在LASD应用中是特别令人感兴趣的。
测量聚合物颗粒的Mn的凝胶渗透色谱方法
基于聚合物固体含量计，在THF中以5mg/mL的浓度制备GPC样品。将样品溶液在室温下保持在平床振荡器上过夜，然后在GPC分析之前通过0.45μm PTFE过滤器(Whatman)过滤。GPC仪器设置由Agilent 1200系列HPLC系统(脱气装置、泵、自动进样器)和Wyatt T-rEX折射率检测器组成。在柱集上进行聚合物分离，所述柱集由一个TOSOH TSKgel GMHxl-L和一个TOSOH TSKgel G5000Hxl柱(每个堆积有9μm苯乙烯二乙烯基苯凝胶；每个尺寸：7.5mmIDx30cm)组成，使用THF作为流动相，流速为1mL/min；进样量为40μL。
Astra 7软件(Wyatt Technology)用于数据采集和处理。使用基于聚苯乙烯标准物(Agilent Technology)的常规校准方法计算Mn和Mw，如下表1所示：
表1：聚苯乙烯标准品
基于聚苯乙烯校准曲线和样品洗脱曲线通过以下等式获得数均分子量和重均分子量：
其中hi是第i个体积增量处的GPC曲线高度，Mi是基于聚苯乙烯校准曲线在第i个滞留体积处洗脱的物质的分子量。
由表2中所示的组分以所列顺序制备含有石蜡或者石蜡与聚乙烯的共混物的涂层配制品。将组分与顶置式搅拌器混合10分钟，然后使其平衡过夜。基于粘合剂固体的重量，添加6.4重量％的蜡。在没有蜡的情况下制备的比较例(表3)使用相同的配制品，但用另外的粘合剂固体代替蜡固体。粘合剂是指Mn为约21,000g/mol的50.5％固体BA 55/MMA 42/PEM 3胶乳。(PEM具有60％的活性。)密度是指干密度。TERGITOL、TAMOL和ACRYSOL是陶氏化学公司(The Dow Chemical Company)或其附属公司的商标。Expancel 031WUF 40是指Expancel 031WUF 40热塑性微球。
表2-具有蜡的涂层配制品
组分 质量(g) 固体(％) 密度(g/cm3)
粘合剂(BA 55/MMA 42/PEM 3) 27.04 50.5 1.1
蜡乳液(固体) 0.87 30-50 0.9
TAMOLTM1254分散剂 0.96 35 2.1
TERGITOLTM15-S-40非离子表面活性剂 0.1 50 1.2
Bayferrox 318M着色剂 0.2 100 4.6
Titan 200碳酸钙 66.64 100 2.7
Kollotex 1500马铃薯淀粉 1.82 100 1.6
Expancel 031WUF 40 0.15 76 1.0
ACRYSOLTMRM-12W流变改性剂 0.12 19 1.27
ACRYSOLTMTT-615流变改性剂 0.08 30 1.23
表3-没有蜡的涂层配制品
水吸收测试
将涂层在铝板上拉伸到4x100x80mm样品中。然后将样品在室温下放置30分钟，随后在150℃下烘焙30分钟。将样品冷却至室温并称重以确定其总质量。然后将样品浸入10cm水中48小时并再次称重。水吸收报告为浸泡和未浸泡样品之间的质量差异百分比。
表4示出了在具有和没有石蜡的情况下涂层(2天后测试的3个板的平均值)的水吸收百分比(WPU％)。ML 190是指Michem Lube 190聚乙烯蜡乳液；Aquacer 593是指Aquacer593聚丙烯蜡乳液；ML 723是指Michem Lube 723石蜡乳液；Aquacer 497是指Aquacer 497石蜡乳液；ME 62330是指Michem 62330石蜡/PE蜡共混物乳液；并且ML 270R是指MichemLube270R石蜡/PE蜡共混物乳液。
对于粘度介于1,000,000厘泊(cP)和10,000,000cP之间的涂层，使用具有Brookfield Helipath支架和T-Bar T-E型转子的Brookfield RV DV-I+粘度计在25℃测量布氏粘度。Brookfield T-Bar T-C型和T-F型转子可以分别用于介于200,000cP和1,000,000cP之间以及介于10,000,000cP和20,000,000cP之间的粘度。转子的旋转速度为0.5rpm，并且转子在进行测量之前运行120秒(即，在无剪切条件下)。该支架允许转子在旋转期间向下移动到涂料中，以确保高粘度材料的正确测量。粘度以厘泊(cP)x 104测量。表4示出了涂层的水吸收数据。
表4-涂层的水吸收结果
该数据表明由含有PE蜡的配制品制备的涂层(比较例2)和由不含蜡的配制品制备的涂层(比较例1)的水吸收没有差异。相比之下，对于由含有石蜡的配制品制备的涂层(实施例1和实施例2)以及含有石蜡和聚乙烯蜡的共混物的配制品制备的涂层(实施例3和实施例4)观察到水吸收的显著降低。

Claims (10)

1.一种组合物，所述组合物包含以下物质的含水分散体：丙烯酸聚合物颗粒，所述丙烯酸聚合物颗粒具有50nm至500nm范围内的z平均粒度和-25℃至30℃范围内的计算Tg；石蜡；增量剂颗粒；和流变改性剂；其中所述组合物的颜料体积浓度在40至70的范围内；并且其中当不在剪切条件下时，所述组合物的布氏粘度在200,000cP至20,000,000cP的范围内。
2.根据权利要求1所述的组合物，其中基于所述组合物的重量，丙烯酸聚合物颗粒的浓度在10重量％至25重量％的范围内；并且基于所述丙烯酸聚合物颗粒的重量，石蜡的浓度在1％至15％的范围内。
3.根据权利要求2所述的组合物，其中所述丙烯酸聚合物颗粒具有在-10℃至20℃范围内的计算Tg，并且包含甲基丙烯酸甲酯和选自以下的一种或多种单体的结构单元：丙烯酸乙酯、丙烯酸丁酯、丙烯酸2-乙基己酯和丙烯酸2-丙基庚酯；并且其中所述组合物的布氏粘度在1,000,000cP至10,000,000cP的范围内。
4.根据权利要求3所述的组合物，其中所述丙烯酸聚合物颗粒还包含甲基丙烯酸磷酸乙酯的结构单元。
5.根据权利要求2所述的组合物，所述组合物还包含聚乙烯蜡或聚丙烯蜡的150个至1500个重复单元，其中基于所述石蜡和所述聚乙烯蜡或所述聚丙烯蜡的重量，所述聚乙烯蜡或所述聚丙烯蜡与所述石蜡的重量比在5重量％至35重量％的范围内。
6.根据权利要求3所述的组合物，所述组合物还包含聚乙烯蜡的150个至1500个重复单元，其中基于所述石蜡和所述聚乙烯蜡的重量，所述聚乙烯蜡与所述石蜡的重量比在5重量％至35重量％的范围内。
7.根据权利要求3所述的组合物，其中所述增量剂颗粒是碳酸钙颗粒。
8.根据权利要求1所述的组合物，所述组合物包含小于5PVC水平的遮光颜料。
9.根据权利要求2所述的组合物，其中所述聚合物颗粒的数均分子量在10,000g/mol至40,000g/mol的范围内。
10.根据权利要求1所述的组合物，所述组合物还包含马铃薯淀粉。
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